CN103616473A - Method for measuring iron content in direct reduction iron of steelmaking auxiliary material - Google Patents
Method for measuring iron content in direct reduction iron of steelmaking auxiliary material Download PDFInfo
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Abstract
The invention discloses a method for measuring the iron content in direct reduction iron of a steelmaking auxiliary material. The method comprises the following steps: 1, decomposing a test sample, namely, weighing a reduced iron test sample, adding an FeCl3 solution, placing on a magnetic stirrer, and stirring for 20-30min; 2, filtering the test sample, namely, filtering and sealing the stirred test sample; and 3, titrating the test sample, namely, adding sulfuric-phosphoric mixed acid in the test sample, sealing a suction filtration bottle opening by using a rubber plug, placing on the magnetic stirrer, stirring for 20-30min, opening the rubber plug of the suction filtration bottle opening, adding 50-60 drops of a 0.2% sodium diphenylaminesulfonate indicator in each 1 g of reduced iron test sample, titrating by using a sodium diphenylaminesulfonate standard solution until the solution is of a stable bluish violet, recording a volume of the consumed potassium dichromate standard solution, and calculating the content of metal iron according to a formula. The method prevents the metal iron from being oxidized, and is good in repeatability and accurate in measurement; the measurement accuracy of test sample testing is within 1.0 percent.
Description
Technical field
The present invention relates to the method for testing of iron-holder, refer to particularly the assay method of all iron content in a kind of steelmaking ingredient DRI.
Technical background
In steel, nonmetallic materials and non-ferrous metal usage ratio increase, and cause waste steel quality constantly to decline.Steel scrap is as steelmaking feed, and because its source is different, chemical component fluctuation is very large, and is difficult to grasp, control, and this has brought great difficulty to steel-making operation.
DRI (DRI-Direct Reduced Iron) is the low-carbon (LC) vesicular material that smart iron powder or iron oxide form through low-temperature reduction in stove, its chemical composition stability, and impurity content is few.DRI is due to chemical composition stability, can effectively dilute remaining in steel and tramp metal constituent content, thereby can improve the quality of steel, and the phosphorus in DRI, sulphur harmful element content are low, add in steel scrap and make steel, can shorten refining time, burn-off rate is fast, energy consumption is low, can raise the efficiency, reduce costs; There is use cost cheap, economic benefit high.Therefore the composition of DRI has significant impact to steel-making quality.With a certain proportion of DRI, as thinning agent and steel scrap collocation, not only can increase the homogeneity of steel, can also improve the physical property of steel, thereby reach the object of production high-quality steel.Therefore, DRI is not only the substitute of high-quality steel scrap, or the requisite senior raw material of production high-quality steel.
Yet, the content of the metallic iron in DRI is not easy to determine, also do not determine at present quantitative analysis, assay method, conventional sampler-dissolving method sample dissolution not exclusively, also the titration measuring error of useful routine is larger, therefore, also do not have at present effective method to measure all iron content in DRI; And in measuring process, for avoiding the oxidation of metallic iron to cause measurement result on the low side, air need to be completely cut off as much as possible, therefore, on-the-spot to sample analysis requirement fast and accurately in order to meet, need to invent a kind of quick and precisely, isolated air measures the method for metal Ferrum content in DRI.
Summary of the invention
Object of the present invention is exactly the assay method that all iron content in a kind of steelmaking ingredient DRI will be provided, and the method operating process is simple, has avoided the oxidation of metallic iron, reproducible, and sample detects measuring accuracy in 1.0%, measures accurately.
For achieving the above object, the assay method of all iron content in the designed steelmaking ingredient DRI of the present invention, comprises the following steps:
1) sample decomposes: taking reduced iron sample and put into closed container, is 8～12% FeCl to adding mass concentration in closed container
3solution, every 1g reduced iron sample adds 250-400mL, described FeCl
3solution was removed dissolved oxygen DO wherein before adding, and then made sample all dissolve;
2) sample filters: under airtight condition, the sample after dissolving is filtered;
3) sample titration: add mixture of sulfuric phosphoric acid in the solution after filtration, every 1g reduced iron sample adds 250-400mL mixture of sulfuric phosphoric acid and 2.5L distilled water, is stirred to abundant dissolving after sealing; In reduced iron sample, add diphenylamine sulfonic acid sodium salt indicator, after mixing, with potassium dichromate standard solution, be titrated to solution and be stable bluish violet under air-tight state, write down the volume of the potassium dichromate standard solution of consumption, according to following formula, calculate the content of metallic iron:
In formula:
The concentration of c-potassium dichromate standard solution, unit: mol/L,
The volume of the potassium dichromate standard solution that V-titration consumes, unit: mL,
M-takes reduced iron sample mass, unit: g.
Further, in described step 1), FeCl
3the preparation process of solution is: take 83gFeCl
36H
2o is dissolved in 500mL cold water, after dissolve complete, and suction filtration, and being transferred in reagent bottle, and the dissolved oxygen DO removed wherein for 1 hour of logical nitrogen.
Further, in described step 3), the preparation process of potassium dichromate standard solution is: take 5.8836g or 11.7672g potassium dichromate primary standard substance, after adding distil water dissolves completely, transfer in 500mL volumetric flask, constant volume, shakes up, and is placed in 500mL reagent bottle.
Again further, in described step 3), the preparation process of diphenylamine sulfonic acid sodium solution is: take 0.2g diphenylamine sulfonic acid sodium salt and be dissolved in 100mL water, add 0.2mL sulfuric acid solution, in sulfuric acid solution, the volume ratio of sulfuric acid and water is 1:1.
Again further, in described step 3), the preparation process of mixture of sulfuric phosphoric acid is: measure 200mL distilled water in 500mL beaker, slowly add the 150mL concentrated sulphuric acid, after cooling, add 150mL strong phosphoric acid, mix, be transferred to 500mL reagent bottle and make the mixture of sulfuric phosphoric acid that sulphur, phosphorus, water volume ratio are 3:3:4.
Again further, described step 2) in, described sample filter process is: in M-50 molding sand core filtering activities device, adopt qualitative filter paper suction filtration, and wash fast filter paper 4-5 times with distilled water, take off M-50 molding sand core filtering activities device, immediately with rubber stopper by bottle sealing.With tongs, by the sealing of suction filtration mouth proofed sleeve, take off bottle,suction.
Again further, in described step 1), it is tool plug conical flask that sample decomposes container used.
Again further, in described step 1), tool plug conical flask is placed in and on magnetic stirring apparatus, stirs 20-30min sample is all dissolved.
The present invention can detect the content range of metallic iron in DRI 20～98%, has almost contained in production run the distribution gradient of metallic iron in DRI, can prolonged application in the quantitative detection of metallic iron.The present invention is in the whole process detecting, completely cut off contacting of sample and air, whole process is close to vacuum state, effectively avoided the oxidational losses of metallic iron in analytic process, accuracy and the precision of analytical approach have greatly been improved, through overtesting, detect, the precision of measurement of detection method of the present invention reaches 1.0%.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail:
Embodiment 1
An assay method for all iron content in steelmaking ingredient DRI, comprises the following steps:
1) sample granularity, blank test and mensuration number of times
1.1) sample granularity: sample granularity should be less than 0.125mm(and be less than 120 orders).
1.2) blank test: do blank test in company with sample, agents useful for same must be taken from same reagent bottle.
1.3) measure number of times: same sample, in same testing laboratory, should be undertaken 2 times by same operator and measure.
1.4) correction test: in company with the close standard model of sample analysis content of the same type.
2) device and reagent
2.1) tool plug conical flask (200mL)
2.2) S21-2 type magnetic stirrer
2.3) M-50 molding sand core filtering activities device
2.4) qualitative filter paper
2.5) bottle,suction (200mL)
2.6) tool plug suction filtration buret
2.7) mixture of sulfuric phosphoric acid (3+3+4): measure 200mL distilled water in 1000mL beaker, slowly add the 300mL concentrated sulphuric acid, cooling after, add 300mL strong phosphoric acid, mix, be transferred to 1000mL reagent bottle, standby.
2.8) liquor ferri trichloridi (10%): take 83gFeCl
36H
2o is dissolved in 500mL cold water, and after dissolve complete, suction filtration, is transferred in reagent bottle, and the dissolved oxygen DO removed wherein for 1 hour of logical nitrogen.
2.9) potassium dichromate standard solution: accurately take 11.7672g potassium dichromate primary standard substance, add after a small amount of distilled water dissolving, transfer in 500mL volumetric flask, constant volume, shakes up, and is placed in 500mL reagent bottle.
2.10) diphenylamine sulfonic acid sodium solution (0.2%): take 0.2g diphenylamine sulfonic acid sodium salt and be dissolved in 100mL water, add 0.2mL sulfuric acid (1+1).
3) sample decomposes
Accurately take 0.2000g reduced iron sample in 200mL tool plug conical flask, add rapidly 60mL to remove the liquor ferri trichloridi of dissolved oxygen DO, cover tightly bottle cap, be placed in and on magnetic stirring apparatus, stir 30min and all dissolve to sample.
4) sample filters
In M-50 molding sand core filtering activities device, adopt qualitative filter paper suction filtration, and wash fast filter paper 4 times with distilled water, take off M-50 molding sand core filtering activities device, immediately with rubber stopper by bottle sealing.With tongs, by the sealing of suction filtration mouth proofed sleeve, take off bottle,suction.
5) sample titration
Open suction filtration bottleneck rubber stopper, add rapidly 60mL mixture of sulfuric phosphoric acid, and 150mL distilled water, immediately with rubber stopper by bottle sealing, be placed on magnetic stirring apparatus.Open suction filtration bottleneck rubber stopper, add 5 diphenylamine sulfonic acid sodium salt indicator, with the tool plug suction filtration buret titration of in-built potassium dichromate standard solution by bottle sealing, open tool plug suction filtration buret water source and carry out suction filtration, turn on agitator, is titrated to solution with potassium dichromate standard solution and is stable bluish violet.Write down the volume of the potassium dichromate standard solution of consumption, according to formula, calculate the content of metallic iron:
In formula: the concentration of c-potassium dichromate standard solution, unit: mol/L,
The volume of the potassium dichromate standard solution that V-titration consumes, unit: mL
M-sample weighting amount, unit: g.
Measurement result is as following table 1, table 2:
Table 1: standard model metallic iron measurement result
As can be seen from Table 1, between standard model Euro MRC685-1 measured value and standard value, difference is 0.075% at 0.31%, RSD, and description standard sample analysis result accuracy and precision are all higher, can carry out the measurement result of metallic iron in sample.
Table 2: sample metallic iron measurement result
As can be seen from Table 2, sample analysis RSD≤0.786%, sample analysis precision is good, can meet need of production.
Embodiment 2
The assay method of all iron content in steelmaking ingredient DRI, comprises the following steps:
1) sample granularity, blank test and mensuration number of times
1.1) sample granularity: sample granularity should be less than 0.125mm(and be less than 120 orders).
1.2) blank test: do blank test in company with sample, agents useful for same must be taken from same reagent bottle.
1.3) measure number of times: same sample, in same testing laboratory, should be undertaken 2 times by same operator and measure.
1.4) correction test: in company with the close standard model of sample analysis content of the same type.
2) device and reagent
2.1) tool plug conical flask (100mL)
2.2) S21-2 type magnetic stirrer
2.3) M-50 molding sand core filtering activities device
2.4) qualitative filter paper
2.5) bottle,suction (500mL)
2.6) tool plug suction filtration buret
2.7) mixture of sulfuric phosphoric acid (3+3+4): measure 200mL distilled water in 500mL beaker, slowly add the 150mL concentrated sulphuric acid, cooling after, add 150mL strong phosphoric acid, mix, be transferred to 500mL reagent bottle, standby.
2.8) liquor ferri trichloridi (10%): take 83gFeCl
36H
2o is dissolved in 500mL cold water, and after dissolve complete, suction filtration, is transferred in reagent bottle, and the dissolved oxygen DO removed wherein for 1 hour of logical nitrogen.
2.9) potassium dichromate standard solution: accurately take 5.8836g potassium dichromate primary standard substance, add after a small amount of distilled water dissolving, transfer in 500mL volumetric flask, constant volume, shakes up, and is placed in 500mL reagent bottle.
2.10) diphenylamine sulfonic acid sodium solution (0.2%): take 0.2g diphenylamine sulfonic acid sodium salt and be dissolved in 100mL water, add 0.2mL sulfuric acid (1+1).
3) sample decomposes
Accurately take 0.1000g reduced iron sample in 100mL tool plug conical flask, add rapidly 30mL to remove the liquor ferri trichloridi of dissolved oxygen DO, cover tightly bottle cap, be placed in and on magnetic stirring apparatus, extract 20min.
4) sample filters
In M-50 molding sand core filtering activities device, adopt qualitative filter paper suction filtration, and wash fast filter paper 5 times with distilled water, take off M-50 molding sand core filtering activities device, immediately with rubber stopper by bottle sealing.With tongs, by the sealing of suction filtration mouth proofed sleeve, take off bottle,suction.5) sample titration
Open suction filtration bottleneck rubber stopper, add rapidly 30mL mixture of sulfuric phosphoric acid, and 250mL distilled water, immediately with rubber stopper by bottle sealing, be placed on magnetic stirring apparatus.Open suction filtration bottleneck rubber stopper, add 6 diphenylamine sulfonic acid sodium salt indicator, with the tool plug suction filtration buret titration of in-built potassium dichromate standard solution by bottle sealing, open tool plug suction filtration buret water source and carry out suction filtration, turn on agitator, is titrated to solution with potassium dichromate standard solution and is stable bluish violet.Write down the volume of the potassium dichromate standard solution of consumption, according to formula, calculate the content of metallic iron:
In formula:
The concentration of c-potassium dichromate standard solution, unit: molL
-1,
The volume of the potassium dichromate standard solution that V-titration consumes, unit: mL
M-sample weighting amount, unit: g.
Measurement result is as following table 3, table 4:
Table 3: standard model metallic iron measurement result
As can be seen from Table 3, between standard model Euro MRC685-1 measured value and standard value, difference is 0.298% at 0.23%, RSD, and description standard sample analysis result accuracy and precision are all higher, can carry out the measurement result of metallic iron in sample.
Table 4: produce sample metallic iron measurement result
As can be seen from Table 4, sample analysis RSD≤0.710%, sample analysis precision is good, can meet need of production.
Embodiment 3
The assay method of all iron content in steelmaking ingredient DRI, comprises the following steps:
1) sample granularity, blank test and mensuration number of times
1.1) sample granularity: sample granularity should be less than 0.125mm(and be less than 120 orders).
1.2) blank test: do blank test in company with sample, agents useful for same must be taken from same reagent bottle.
1.3) measure number of times: same sample, in same testing laboratory, should be undertaken 2 times by same operator and measure.
1.4) correction test: in company with the close standard model of sample analysis content of the same type.
2) device and reagent
2.1) tool plug conical flask (100mL)
2.2) S21-2 type magnetic stirrer
2.3) M-50 molding sand core filtering activities device
2.4) qualitative filter paper
2.5) bottle,suction (500mL)
2.6) tool plug suction filtration buret
2.7) mixture of sulfuric phosphoric acid (3+3+4): measure 200mL distilled water in 500mL beaker, slowly add the 150mL concentrated sulphuric acid, cooling after, add 150mL strong phosphoric acid, mix, be transferred to 500mL reagent bottle, standby.
2.8) liquor ferri trichloridi (10%): take 83gFeCl
36H
2o is dissolved in 500mL cold water, and after dissolve complete, suction filtration, is transferred in reagent bottle, and the dissolved oxygen DO removed wherein for 1 hour of logical nitrogen.
2.9) potassium dichromate standard solution: accurately take 5.8836g potassium dichromate primary standard substance, add after a small amount of distilled water dissolving, transfer in 500mL volumetric flask, constant volume, shakes up, and is placed in 500mL reagent bottle.
2.10) diphenylamine sulfonic acid sodium solution (0.2%): take 0.2g diphenylamine sulfonic acid sodium salt and be dissolved in 100mL water, add 0.2mL sulfuric acid (1+1).
3) sample decomposes
Accurately take 0.4000g reduced iron sample in 100mL tool plug conical flask, add rapidly 30mL to remove the liquor ferri trichloridi of dissolved oxygen DO, cover tightly bottle cap, be placed in and on magnetic stirring apparatus, extract 20min.
4) sample filters
In M-50 molding sand core filtering activities device, adopt qualitative filter paper suction filtration, and wash fast filter paper 5 times with distilled water, take off M-50 molding sand core filtering activities device, immediately with rubber stopper by bottle sealing.With tongs, by the sealing of suction filtration mouth proofed sleeve, take off bottle,suction.5) sample titration
Open suction filtration bottleneck rubber stopper, add rapidly 30mL mixture of sulfuric phosphoric acid, and 250mL distilled water, immediately with rubber stopper by bottle sealing, be placed on magnetic stirring apparatus.Open suction filtration bottleneck rubber stopper, add 6 diphenylamine sulfonic acid sodium salt indicator, with the tool plug suction filtration buret titration of in-built potassium dichromate standard solution by bottle sealing, open tool plug suction filtration buret water source and carry out suction filtration, turn on agitator, is titrated to solution with potassium dichromate standard solution and is stable bluish violet.Write down the volume of the potassium dichromate standard solution of consumption, according to formula, calculate the content of metallic iron:
In formula:
The concentration of c-potassium dichromate standard solution, unit: molL
-1,
The volume of the potassium dichromate standard solution that V-titration consumes, unit: mL
M-sample weighting amount, unit: g.
Measurement result is as following table 5
Table 5: produce sample metallic iron measurement result
As can be seen from Table 5, sample analysis RSD≤0.829%, sample analysis precision is good, can meet need of production.
Claims (8)
1. an assay method for all iron content in steelmaking ingredient DRI, comprises the following steps:
1) sample decomposes: taking reduced iron sample and put into closed container, is 8～12% FeCl to adding mass concentration in closed container
3solution, every 1g reduced iron sample adds 250-400mL, described FeCl
3solution was removed dissolved oxygen DO wherein before adding, and then made sample all dissolve;
2) sample filters: under airtight condition, the sample after dissolving is filtered;
3) sample titration: add mixture of sulfuric phosphoric acid in the solution after filtration, every 1g reduced iron sample adds 250-400mL mixture of sulfuric phosphoric acid and 2.5L distilled water, is stirred to abundant dissolving after sealing; In reduced iron sample, add diphenylamine sulfonic acid sodium salt indicator, after mixing, with potassium dichromate standard solution, be titrated to solution and be stable bluish violet under air-tight state, write down the volume of the potassium dichromate standard solution of consumption, according to following formula, calculate the content of metallic iron:
In formula:
The concentration of c-potassium dichromate standard solution, unit: mol/L,
The volume of the potassium dichromate standard solution that V-titration consumes, unit: mL,
M-takes reduced iron sample mass, unit: g.
2. the assay method of all iron content in steelmaking ingredient DRI according to claim 1, is characterized in that: in described step 1), and FeCl
3the preparation process of solution is: take 83gFeCl
36H
2o is dissolved in 500mL cold water, and after dissolve complete, suction filtration, and being transferred in reagent bottle, and the dissolved oxygen DO removed wherein for 1 hour of logical nitrogen, obtain mass concentration and be 10% FeCl
3solution.
3. according to the assay method of all iron content in steelmaking ingredient DRI described in claim 1 or 2, it is characterized in that: in described step 3), the preparation process of potassium dichromate standard solution is: take 5.8836g or 11.7672g potassium dichromate primary standard substance, after adding distil water dissolves completely, transfer in 500mL volumetric flask, constant volume, shakes up, and is placed in 500mL reagent bottle.
4. according to the assay method of all iron content in steelmaking ingredient DRI described in claim 1 or 2, it is characterized in that: in described step 3), the preparation process of diphenylamine sulfonic acid sodium solution is: take 0.2g diphenylamine sulfonic acid sodium salt and be dissolved in 100mL water, add 0.2mL sulfuric acid solution, in sulfuric acid solution, the volume ratio of sulfuric acid and water is 1:1.
5. according to the assay method of all iron content in steelmaking ingredient DRI described in claim 1 or 2, it is characterized in that: in described step 3), the preparation process of mixture of sulfuric phosphoric acid is: measure 200mL distilled water in 500mL beaker, slowly add the 150mL concentrated sulphuric acid, after cooling, add 150mL strong phosphoric acid, mix, be transferred to 500mL reagent bottle and make the mixture of sulfuric phosphoric acid that sulphur, phosphorus, water volume ratio are 3:3:4.
6. according to the assay method of all iron content in steelmaking ingredient DRI described in claim 1 or 2, it is characterized in that: described step 2), described sample filter process is: in M-50 molding sand core filtering activities device, adopt qualitative filter paper suction filtration, and wash fast filter paper 4-5 times with distilled water, take off M-50 molding sand core filtering activities device, immediately with rubber stopper by bottle sealing.With tongs, by the sealing of suction filtration mouth proofed sleeve, take off bottle,suction.
7. the assay method of all iron content in steelmaking ingredient DRI according to claim 3, is characterized in that: in described step 1), it is tool plug conical flask that sample decomposes container used.
8. the assay method of all iron content in steelmaking ingredient DRI according to claim 7, is characterized in that: in described step 1), tool plug conical flask is placed in and on magnetic stirring apparatus, stirs 20-30min sample is all dissolved.
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| CN105067754A (en) * | 2015-07-30 | 2015-11-18 | 武汉钢铁(集团)公司 | Method for analyzing content of iron in hot-dip galvanized alloyed steel plate by oxidimetry |
| CN112924616A (en) * | 2019-12-05 | 2021-06-08 | 中核四0四有限公司 | Method for measuring total reduction value in post-treatment process feed liquid |
| CN112946171A (en) * | 2021-01-18 | 2021-06-11 | 浙江华恒交通建设监理有限公司 | Full-automatic EDTA titration detection method |
| CN114924027A (en) * | 2022-03-31 | 2022-08-19 | 天津钢铁集团有限公司 | Method for measuring content of metallic iron in iron scale |
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| CN112946171A (en) * | 2021-01-18 | 2021-06-11 | 浙江华恒交通建设监理有限公司 | Full-automatic EDTA titration detection method |
| CN114924027A (en) * | 2022-03-31 | 2022-08-19 | 天津钢铁集团有限公司 | Method for measuring content of metallic iron in iron scale |
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| Publication number | Publication date |
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| CN103616473B (en) | 2016-09-14 |
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